PtRu bimetallic nanoparticles supported on carbon nanoparticle (PtRu/C) catalysts were synthesized with radiation irradiation. The samples were structural analyzed by techniques of X-ray absorption fine structure (XAFS), transmission electron microscope (TEM) and X-ray diffraction (XRD). The results indicated that PtRu/C catalysts which prepared by an electron beam irradiation had more homogeneous atomic arrangement than that prepared by a gamma-ray irradiation. We found a clear correlation between the atomic structure and the catalytic activity of PtRu/C catalysts. These results supported the bi-functional mechanism.